8IVR

Methyl and Fluorine Effects in Novel Orally Bioavailable Keap1/Nrf2 PPI Inhibitor for Treatment of Chronic Kidney Disease

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SLS BEAMLINE X06SA
Synchrotron site	SLS
Beamline	X06SA
Temperature [K]	100
Detector technology	PIXEL
Collection date	2014-04-10
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1.0
Spacegroup name	P 61
Unit cell lengths	103.911, 103.911, 54.425
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	89.990 - 1.500
R-factor	0.1824
Rwork	0.182
R-free	0.19790
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.002
RMSD bond angle	0.554
Data reduction software	XDS
Data scaling software	Aimless
Phasing software	PHASER
Refinement software	PHENIX (1.20_4459)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	89.990	1.540
High resolution limit [Å]	1.500	1.500
Rmerge	0.082	0.351
Number of reflections	52857	3800
<I/σ(I)>	17.1	4
Completeness [%]	98.4
Redundancy	8.9

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION	7.5	277	hKEAP1 was concentrated to 6-10 mg/mL and crystallized with the solution with 0.1M Na acetate (pH5.0) and 1.5M di-ammonium sulfate or the solution with 0.1M Na acetate (pH5.0), 1.5M di-ammonium, and 0.1-0.15M NaCl